CN103088418A - Crystalline silicon ingot and its making method - Google Patents
Crystalline silicon ingot and its making method Download PDFInfo
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- CN103088418A CN103088418A CN2011103375123A CN201110337512A CN103088418A CN 103088418 A CN103088418 A CN 103088418A CN 2011103375123 A CN2011103375123 A CN 2011103375123A CN 201110337512 A CN201110337512 A CN 201110337512A CN 103088418 A CN103088418 A CN 103088418A
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Abstract
The invention discloses a crystalline silicon ingot and its making method. The large-dimension silicon grain distribution proportion is greatly reduced through thermal field parameter control, the dense covering of nucleating sites on the bottom of a crucible and the like. The average grain dimension of silicon grains at the bottom of the silicon ingot is less than 12mm, and the average grain dimension of the silicon grains in the upper area of the silicon ingot is greater than 14mm. Small-dimension silicon grains has a less grain competition phenomenon in the nucleation process, has a dense distribution, and has a single upward growth trend, so the big-eating-small situation of grains is reduced, and the incomplete columnar crystal growth is avoided. Additionally, the grain boundaries having a highly dense distribution provide channels for smoothly moving dislocations or other stress defects in crystals, so the defect increase rate is reduced, thereby the crystalline silicon ingot integrally has a good crystal quality, and the photoelectric conversion efficiency of a solar battery subsequently made in the invention is high.
Description
Technical field
The present invention relates to a kind of silicon crystal ingot (crystalline silicon ingot) and manufacture method thereof, and especially, be that small size silicon crystal grain and top are silicon crystal ingot and the manufacture method thereof of large size silicon crystal grain about its bottom.
Background technology
Background of related of the present invention please refer to following listed document:
[1] K.Fujiwara, W.Pan, K.Sawada, M.Tokairin, N.Usami, Y.Nose, A.Nomura, T.Shishida, K.Nakajima. " Directional growth method to obtain high quality polycrystalline silicon from its melt " .Journal of Crystal Growth 2006; (the K. rattan is former, Pan W., field, K. pool, M.Tokairin, N. Sa rice, Y. Moses 《Sheng Jing》Zhong Xibailairenxianzhiming, A. open country village, T.Shishida, island in K. for 292:282-285." method of oriented growth obtains the high-quality polysilicon of its melt." the crystal growth magazine of 2006 years; 292:282-285); And
[2] T.Y.Wang, S.L.Hsu, C.C.Fei, K.M.Yei, W.C.Hsu, C.W.Lan. " Grain control using spot cooling in multi-crystalline silicon crystal growth " .Journal of Crystal Growth 2009; 311:263-267 (T.Y. king, S.L. is permitted, and C.C. takes, the K.M. leaf, W.C. is permitted, and C.W. is blue." grain is controlled and is used the cooling of polycrystal silicon crystal growth then and there ".The China's crystal of 2009 growth magazine; 311:263-267).
The long crystalline substance of laboratory grade polycrystalline silicon casting can reach at crucible (crucible) bottom control growth crystal face dendritic crystal (facet dendrite).For example, it is horizontal long brilliant that above-mentioned reference [1] proposes to utilize local overcooling (undercooling) first to be covered with in crucible bottom, the columnar structure of upwards growing up again, its large size silicon crystal grain has fabricating low-defect-density (defect density) and better twin crystal structure (sigma 3).Therefore, according to the silicon crystal ingot that document [1] is made, its Silicon Wafer after section is made solar cell, can obtain higher photoelectric transformation efficiency.
Yet when extending to the technical grade size, the polysilicon casting is wanted to grow up to be covered with in crucible bottom with local overcooling control crystal face dendritic crystal to become comparatively difficult.The casting of industrial level polysilicon is subject to the impact of crucible and whole being heated evenly property, increase the control variation of initial condensate depression, easily make polysilicon grow into large crystal grain and the better twin crystal structure of nothing in crucible bottom, and become defect concentration higher zone, increase more fast defect concentration when growing up extension, cause silicon crystal ingot bulk crystal degradation, the photoelectric transformation efficiency of the follow-up solar cell of making is also lower.
Summary of the invention
In order to overcome defects, the invention provides a kind of silicon crystal ingot and manufacture method thereof, described silicon crystal ingot and manufacture method thereof can reduce defective advances the speed, and then allows silicon crystal ingot integral body that better crystal mass is arranged, and the photoelectric transformation efficiency of the follow-up solar cell of making is also higher.
The present invention for the technical scheme that solves its technical problem and adopt is:
A kind of silicon crystal ingot, has a bottom, and will be defined as vertical direction with the direction of described bottom vertical, described silicon crystal ingot comprises several silicon crystal grains of growing up along described vertical direction, the average grain size of the silicon crystal grain at place, described bottom is defined as the first average grain size, and described the first average grain size is less than 12mm.
Described silicon crystal ingot is defined as upper zone apart from the position of its bottom 250mm, the average grain size of the silicon crystal grain in described upper zone is defined as the second average grain size, described the second average grain size is greater than 14mm.And described the first average grain size is preferably less than 8mm.
The silicon crystal grain in the described upper zone of described silicon crystal ingot has a defect concentration, and described defect concentration is less than 20% when representing with the defect area ratio.
The manufacture method of above-mentioned silicon crystal ingot, carry out in the steps below:
1., form the molten soup of a silicon in a crucible, will be defined as vertical direction with the perpendicular direction in the bottom of described crucible;
2., control at least one the thermal field parameter about the molten soup of described silicon, cause some silicon crystal grains of growing up from the molten soup of described silicon, described silicon crystal grain is in the bottom interior wall nucleation of described crucible and grow up along described vertical direction;
3., continue to control described at least one thermal field parameter, until the molten soup of described silicon all solidifies to obtain described silicon crystal ingot, the average grain size of the silicon crystal grain at the place, bottom of wherein said silicon crystal ingot is less than 12mm.
The described bottom interior wall of described crucible has the roughness of 300 μ m to 1000 μ m, causes at described bottom interior wall place and offers several nucleation sites of described silicon crystal grain.Be preferably, have some emergences on the described bottom interior wall of described crucible, described some emergences are as several nucleation sites of silicon crystal grain and cause the roughness of the described bottom interior wall of described crucible.Wherein, a kind of in the sintered compact of the green compact body of the sintered compact of described each emergence green compact body that is stupalith, stupalith, graphite and graphite.Wherein, described stupalith is selected from SiN, Si
3N
4, SiO
2, SiC, Al
2O
3A kind of with in AlN.Also can be before silicon crystal ingot be made, first apply sandblasting with the described roughness of the described bottom interior wall that causes described crucible in the described bottom interior wall of described crucible.
Be provided with the well heater that is placed in described crucible top and the directional solidification piece that is placed in described crucible below, described at least one thermal field parameter refer to from described well heater to described crucible the first thermograde (need be controlled at lower than 0.4 ℃/cm), from second thermograde at bottom to the top of described directional solidification piece of the molten soup of described silicon (need be controlled at higher than 17 ℃/cm) and hot propagated flux (need be controlled at higher than 37000W/m
2) at least one.
The invention has the beneficial effects as follows: the difference of the present invention and prior art is, casting proposes to control the methods such as thermal field parameter (thermal control parameter), the densely covered crucible bottom of nucleation site (nucleation site) for polysilicon in the present invention, reduces in a large number large size silicon crystal grain distribution proportion; Because small size silicon crystal grain kenel has less crystal grain warfare in long brilliant process, and the small size silicon crystal grain distributes and closely more easily is tending towards single and upwards grows up, and reduces that crystal grain gobbles little situation and to avoid column crystal to grow up complete; In addition, the densely covered high crystal boundary (grain boundary) that distributes further provides crystal interpolation row (dislocation) or other stress defectives to be able to mobile smoothly pipeline, reducing defective advances the speed, and then allowing silicon crystal ingot integral body that better crystal mass is arranged, the photoelectric transformation efficiency of the follow-up solar cell of making is also higher.
Description of drawings
Fig. 1 is one of the schematic diagram of the manufacture method of the described silicon crystal ingot of the embodiment of the present invention;
Fig. 2 be the described silicon crystal ingot of the embodiment of the present invention manufacture method schematic diagram two;
Fig. 3 is the metallograph of the bottom interior wall of crucible of the present invention, shows to form a plurality of emergences on its bottom interior wall;
Fig. 4 is the metallograph that the bottom interior wall of crucible does not process.
Fig. 5 is the silicon crystal grain size comparative result figure according to the silicon crystal ingot of the silicon crystal ingot of specific embodiment of the invention manufacturing and prior art in contrast;
Fig. 6 is the defect concentration comparative result figure according to the silicon crystal ingot of the silicon crystal ingot of specific embodiment of the invention manufacturing and prior art in contrast;
Fig. 7 is for showing the metallograph of its silicon crystal grain size according to its bottom section of silicon crystal ingot of specific embodiment of the invention manufacturing;
Fig. 8 is the metallograph according to its middle its silicon crystal grain size of zone demonstration of silicon crystal ingot of specific embodiment of the invention manufacturing;
Fig. 9 is for showing the metallograph of its silicon crystal grain size according to its top area of silicon crystal ingot of specific embodiment of the invention manufacturing;
Figure 10 is for showing the metallograph of its defect concentration according to its bottom section of silicon crystal ingot of specific embodiment of the invention manufacturing;
Figure 11 is the metallograph according to its middle its defect concentration of zone demonstration of silicon crystal ingot of specific embodiment of the invention manufacturing;
Figure 12 is for showing the metallograph of its defect concentration according to its top area of silicon crystal ingot of specific embodiment of the invention manufacturing;
Figure 13 is the metallograph that its bottom section of silicon crystal ingot of prior art in contrast shows its silicon crystal grain size;
Figure 14 is the metallograph of its middle its silicon crystal grain size of zone demonstration of silicon crystal ingot of prior art in contrast;
Figure 15 is the metallograph that its top area of silicon crystal ingot of prior art in contrast shows its silicon crystal grain size;
Figure 16 is the metallograph that its bottom section of silicon crystal ingot of prior art in contrast shows its defect concentration;
Figure 17 is the metallograph of its middle its defect concentration of zone demonstration of silicon crystal ingot of prior art in contrast;
Figure 18 is the metallograph that its top area of silicon crystal ingot of prior art in contrast shows its defect concentration;
Figure 19 is the follow-up average light photoelectric transformation efficiency comparative result figure that makes solar cell of silicon crystal ingot according to the silicon crystal ingot of specific embodiment of the invention manufacturing and prior art in contrast.
Description of reference numerals:
1---the long brilliant stove 10 of DSS---body of heater
11---rare gas element conduit 12---adiabatic cage
122---upper heat screen 124---lower heat-insulating shield
14---well heater 16---crucible
162---bottom interior wall 17---pedestal
18---directional solidification piece 19---pillar stiffener
20---silicon melts soup 22---silicon crystal grain
V---vertical direction.
Embodiment
Embodiment: this example provides a kind of silicon crystal ingot manufacture method, it controls thermal field parameter (thermal control parameter), the densely covered crucible bottom of nucleation site (nucleation site) etc., reduces in a large number large size silicon crystal grain distribution proportion.And made silicon crystal ingot integral body has better crystal mass, and the photoelectric transformation efficiency of the follow-up solar cell of making is also higher.
See also Fig. 1 and Fig. 2, schematically illustrate the method for the manufacturing silicon crystal ingot of the embodiment of the present invention.
As shown in Figure 1, manufacture method of the present invention is followed directional solidification system (directional solidification system, DSS) haply, adopts the long brilliant stove 1 of a DSS.The adiabatic cage 12 that the structure of the long brilliant stove 1 of this DSS comprises a body of heater 10, be made of heat screen 122 on one and heat-insulating shield 124 once, be placed in a directed cured block 18 in this thermal insulation cage 12, support at least one pillar stiffener 19 of this directional solidification piece 18, a rare gas element conduit 11 that is placed in a pedestal 17 on this directional solidification piece 18, is placed in a crucible 16 in this pedestal 17, is placed in the well heater 14 on this crucible and connects this body of heater 10 and this thermal insulation cage 12.
On practice, this crucible 16 can be quartz crucible.This directional solidification piece 18 can be made by graphite.This pedestal 17 can be made by graphite.This rare gas element conduit 11 is in order to import argon gas to this thermal insulation cage 12.
At first method of the present invention is at the molten soup 20 of interior formation one silicon of this crucible 16, as shown in Figure 1.This crucible 16 itself defines a vertical direction V.
Then, control at least one thermal field parameter about the molten soup 20 of this silicon, cause from the molten soup 20 of this silicon a plurality of silicon crystal grains 22 in bottom interior wall 162 nucleation of this crucible 16, and grow up along this vertical direction V, as shown in Figure 2.At least one thermal field parameter comprises a hot propagated flux.As shown in Figure 2, the long brilliant stove 1 of this DSS is in long brilliant process, and heat screen 122 risings on this make to be subjected to the enclosed space that this thermal insulation cage 12 shrouds to produce the gap originally, and this gap just becomes the pipeline of 12 inside and outside heat exchanges of this thermal insulation cage, produces this hot propagated flux.
At last, continue to control this at least one thermal field parameter, all solidify until this silicon melts soup 20, to obtain this silicon crystal ingot.
This bottom interior wall 162 of this crucible 16 has scope from the roughness of 300 μ m to 1000 μ m, causes at this bottom interior wall 162 places and offers a plurality of nucleation sites of these silicon crystal grains.
On practice, cause this bottom interior wall 162 of this crucible 16 to have scope from the method for the roughness of 300 μ m to 1000 μ m, can form in advance a plurality of emergences (protrusion) on this bottom interior wall 162 of this crucible 16, as these a plurality of nucleation sites and cause the above-mentioned roughness of this bottom interior wall 162 of this crucible 16.Each emergence is base substrate in all one's life (green body) or a sintered compact (sintered body) of a stupalith or a graphite.The stupalith of above-mentioned formation emergence can be SiN, Si
3N
4, SiO
2, SiC, Al
2O
3, the fusing point such as AlN is higher than the stupalith of the fusing point of silicon.The processing procedure that forms emergence can be modulated into slurries with the powder of powdered graphite or above-mentioned stupalith, slurries is sprayed on this bottom interior wall 162 of this crucible 16, can form the aggregate of above-mentioned powder.Again the aggregate of powder is calcined or sintering procedure according to the calcining temperature, the sintering temperature that are fit to the formation powder, can be formed green compact body or sintered compact as above-mentioned emergence.
In a real case, in above-mentioned spraying process, the pressure of spraying can be controlled in 40～60psi, and the pressure of slurry can be controlled in 15～30psi, and the spraying temperature span of control is 40～60 ℃.Be showed in Fig. 3 according to this real case and the metallograph of bottom interior wall 162 that carries out the crucible 16 of calcination procedure.As contrast, the metallograph that the bottom interior wall 162 of this crucible 16 is not carried out spray procedure is showed in Fig. 4.The metallograph of Fig. 4 shows the bottom interior wall 162 of the crucible 16 that does not carry out spray procedure, and its roughness is 50 μ m～100 μ m.The metallograph of Fig. 3 shows the bottom interior wall 162 of the crucible 16 that carries out spray procedure, calcination procedure, and its roughness is 300 μ m～500 μ m.
Also can adopt different ways, can apply in advance a sandblasting as the bottom interior wall 162 of this crucible 16, cause the bottom interior wall 162 of this crucible 16 to have scope from the roughness of 300 μ m to 1000 μ m.
Please again consult Fig. 1 and Fig. 2, this well heater 14 is the tops that are placed in this crucible 16.This directional solidification piece 18 is the belows that are placed in this crucible 16, indirectly contacts with this crucible 16.This at least one thermal field parameter can comprise from this well heater 14 to this crucible 16 one first thermograde and from one second thermograde at bottom to the top of this directional solidification piece 18 of the molten soup 20 of this silicon or a hot propagated flux etc. thermal field parameter.On practice, this thermograde need be controlled at lower than 0.4 ℃/cm, can be by strengthening the distance between this well heater 14 and this crucible 16, maybe with the heating and temperature control of this well heater 14 lower than 1410 ℃, reach etc. method.This second thermograde need be controlled at higher than 17 ℃/cm, can by strengthening the thickness of this directional solidification piece 18, reach etc. method.This hot propagated flux need be controlled at higher than 37000W/m
2, can by should go up heat screen 122 open speed be promoted to 3cm/hr with on reach.The main purpose of controlling above-mentioned this second thermograde and this hot propagated flux is to increase the condensate depression of the bottom of this crucible 16.
Different from prior art, the first average grain size size of the silicon crystal grain at a bottom place of silicon crystal ingot of the present invention is less than about 12mm.This silicon crystal ingot apart from its bottom approximately the second average grain size of the silicon crystal grain in the upper zone of 250mm greater than about 14mm.The first average grain size preferred range of the silicon crystal grain at place, the bottom of this silicon crystal ingot is less than about 8mm.
The silicon crystal grain in the upper zone of silicon crystal ingot of the present invention has a defect concentration, and this defect concentration represents less than approximately 20% with the defect area ratio.
See also Fig. 5, the A ingot casting is silicon crystal ingot of the present invention, and its average grain size variation along with the silicon crystal ingot height is shown in Fig. 5.Indicate its average grain size along with the silicon crystal ingot height change of B ingot casting in Fig. 5, as contrast.The B ingot casting is the silicon crystal ingot of the method manufacturing that proposes according to document [1].
See also Fig. 6, the corner regions of A ingot casting, sidewall areas and middle section are along with the defect concentration of silicon crystal ingot height change is shown in Fig. 6.Defect concentration in Fig. 6 is to represent with the defect area ratio.As contrast, the corner regions of B ingot casting, sidewall areas and middle section are along with the defect area ratio of silicon crystal ingot height change also is shown in Fig. 6.
See also Fig. 7 to Figure 18, the bottom section of corresponding A ingot casting, region intermediate and top area, the metallograph that shows its silicon crystal grain size is shown in Fig. 7, Fig. 8 and Fig. 9, the bottom section of corresponding A ingot casting, region intermediate and top area (distance A ingot casting bottom approximately 250mm) show that the metallograph of its defect concentration is shown in Figure 10, Figure 11 and Figure 12.As contrast, bottom section, region intermediate and the top area of corresponding B ingot casting, the metallograph that shows its silicon crystal grain size is shown in Figure 13, Figure 14 and Figure 15, bottom section, region intermediate and the top area of corresponding B ingot casting (apart from the about 250mm in B ingot casting bottom) shows that the metallograph of its defect concentration is shown in Figure 16, Figure 17 and Figure 18.
See also Figure 19, the photoelectric transformation efficiency of the made solar cell of bottom section, region intermediate and the top area of the A ingot casting that has drawn from (distance A ingot casting bottom approximately 250mm) is shown in Figure 19.As contrast, the photoelectric transformation efficiency of the made solar cell of bottom section, region intermediate and the top area of the B ingot casting that has drawn from (apart from the about 250mm in B ingot casting bottom) also is shown in Figure 19.
From the data of Fig. 5, Fig. 6 and Figure 19 and the metallograph of Fig. 7 to Figure 18, can know that the brilliant process of length of understanding the B ingot casting grows into large crystal grain and without better twin crystal structure in crucible bottom, and become defect concentration higher zone, increase more fast defect concentration when growing up extension, cause silicon crystal ingot bulk crystal degradation, the photoelectric transformation efficiency of its follow-up solar cell of making is lower.Compared to the B ingot casting, the long brilliant methods such as controlling thermal field parameter, the densely covered crucible bottom of nucleation site of utilizing of A ingot casting reduces large size silicon crystal grain distribution proportion in a large number.Because, small size silicon crystal grain kenel has less crystal grain warfare in long brilliant process, and the small size silicon crystal grain distributes and closely more easily is tending towards single and upwards grows up, and reduces that crystal grain gobbles little situation and to avoid column crystal to grow up complete.In addition, the densely covered high crystal boundary that distributes in the A ingot casting further provides crystal interpolation row or other stress defectives to be able to mobile smoothly pipeline, reduce defective and advance the speed, and then allow silicon crystal ingot integral body that better crystal mass is arranged, the photoelectric transformation efficiency of the follow-up solar cell of making is also higher.
By the above detailed description of preferred embodiments, be to wish more know to describe feature of the present invention with spiritual, and be not with above-mentioned disclosed preferred embodiment to of the present invention towards being limited.On the contrary, its objective is hope can contain the wish application of being arranged in of various changes and tool equality institute of the present invention the scope of the claims towards interior.Therefore, the scope of the claims that the present invention applies for towards doing the broadest explanation according to above-mentioned explanation, contain the arrangement of all possible change and tool equality to cause it.
Claims (12)
1. silicon crystal ingot, has a bottom, and will be defined as vertical direction with the direction of described bottom vertical, it is characterized in that: described silicon crystal ingot comprises several silicon crystal grains of growing up along described vertical direction, the average grain size of the silicon crystal grain at place, described bottom is defined as the first average grain size, and described the first average grain size is less than 12mm.
2. silicon crystal ingot according to claim 1, it is characterized in that: with described silicon crystal ingot apart from its bottom 250mm the position be defined as upper zone, the average grain size of the silicon crystal grain in described upper zone is defined as the second average grain size, and described the second average grain size is greater than 14mm.
3. silicon crystal ingot according to claim 2, it is characterized in that: described the first average grain size is less than 8mm.
4. silicon crystal ingot according to claim 2, it is characterized in that: the silicon crystal grain in the described upper zone of described silicon crystal ingot has a defect concentration, and described defect concentration is less than 20% when representing with the defect area ratio.
5. the manufacture method of silicon crystal ingot according to claim 1, is characterized in that, carries out in the steps below:
1., form the molten soup of a silicon in a crucible, will be defined as vertical direction with the perpendicular direction in the bottom of described crucible;
2., control at least one the thermal field parameter about the molten soup of described silicon, cause some silicon crystal grains of growing up from the molten soup of described silicon, described silicon crystal grain is in the bottom interior wall nucleation of described crucible and grow up along described vertical direction;
3., continue to control described at least one thermal field parameter, until the molten soup of described silicon all solidifies to obtain described silicon crystal ingot, the average grain size of the silicon crystal grain at the place, bottom of wherein said silicon crystal ingot is less than 12mm.
6. the manufacture method of silicon crystal ingot according to claim 5, it is characterized in that: the described bottom interior wall of described crucible has the roughness of 300 μ m to 1000 μ m.
7. the manufacture method of silicon crystal ingot according to claim 6, it is characterized in that: have some emergences on the described bottom interior wall of described crucible, described some emergences are as several nucleation sites of silicon crystal grain and cause the roughness of the described bottom interior wall of described crucible.
8. the manufacture method of silicon crystal ingot according to claim 7 is characterized in that: a kind of in the green compact body of the green compact body that described each emergence is stupalith, the sintered compact of stupalith, graphite and the sintered compact of graphite.
9. the manufacture method of silicon crystal ingot according to claim 8, it is characterized in that: described stupalith is selected from SiN, Si
3N
4, SiO
2, SiC, Al
2O
3A kind of with in AlN.
10. the manufacture method of silicon crystal ingot according to claim 6 is characterized in that: before silicon crystal ingot is made, first apply sandblasting with the described roughness of the described bottom interior wall that causes described crucible in the described bottom interior wall of described crucible.
11. the manufacture method of silicon crystal ingot according to claim 5, it is characterized in that: be provided with the well heater that is placed in described crucible top and the directional solidification piece that is placed in described crucible below, described at least one thermal field parameter refer to from described well heater to described crucible the first thermograde, from the bottom of the molten soup of described silicon to second thermograde at the top of described directional solidification piece and at least one hot propagated flux.
12. the manufacture method of silicon crystal ingot according to claim 11 is characterized in that: described the first thermograde need be controlled at lower than 0.4 ℃/cm; Described the second thermograde need be controlled at higher than 17 ℃/cm; Described hot propagated flux need be controlled at higher than 37000W/m
2
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| CN107208308A (en) * | 2015-02-05 | 2017-09-26 | 瓦克化学股份公司 | The method for preparing polysilicon |
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| CN104609893A (en) * | 2015-01-30 | 2015-05-13 | 扬州荣德新能源科技有限公司 | Method of spraying silicon nitride on inner surface of efficient crucible |
| CN107208308A (en) * | 2015-02-05 | 2017-09-26 | 瓦克化学股份公司 | The method for preparing polysilicon |
| CN107208308B (en) * | 2015-02-05 | 2020-05-15 | 瓦克化学股份公司 | Method for preparing polycrystalline silicon |
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